Separation technology

a technology of separation technology and unsaturated fats, applied in the field of separation technology, can solve the problems of difficult separation of unsaturated fats and fat derivatives from saturated fats and fat derivatives, difficult concentration of unsaturated components in the form of parent triglycerides, and use of non-food grade organic hydrocarbon solvents such as hexane in the extraction process, so as to reduce the pressure of the near-critical fluid phase

Inactive Publication Date: 2010-05-04
IND RES LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

[0019](c) reducing the pressure of the near-critical fluid phase to recover the lipophilic compound.
[0034](e) reducing the pressure of the near-critical fluid phase to recover the fatty acid.
[0047](i) reducing the pressure of the near-critical fluid phase to recover the lipophilic compound.

Problems solved by technology

Separation of unsaturated fats and fat derivatives from saturated fats and fat derivatives is difficult because the unsaturated components are susceptible to thermal and oxidative degradation and because their physical properties do not differ from those of the saturated components [3].
The concentration of the unsaturated components in the form of parent triglycerides is more difficult, because the fatty acids are randomly arranged on the glycerol backbone of the triglyceride [3].
The use of non-food grade organic hydrocarbon solvents such as hexane in the extraction of PUFA or derivatives from the filtrate obtained following urea fractionation of a mixture of FFA or fatty acid derivatives is undesirable, particularly where the product is intended for use as a dietary supplement.
Furthermore, their solubility increases at fixed temperature and pressure when ethanol is added to supercritical CO2 [5].
Known methods for employing supercritical fluids in combination with urea to separate PUFA or their derivatives from mixtures with other fatty acids or derivatives are batch-wise processes, with consequent low production rates.
However, the specification does describe the use of ethanol as a co-solvent which, undesirably, caused urea to precipitate in the valves of the equipment.
However, this method of processing does not eliminate the need for organic hydrocarbon solvents or ensure that hydrocarbon solvent residues can be completely removed.

Method used

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  • Separation technology
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Examples

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Effect test

example 1

Separation of Urea, Glycerol, Salts and FFA

[0172]This example demonstrates the process for recovering FFA from the conversion of fish oil triglycerides to FFA followed directly by urea complexation.

[0173]Ling liver oil (1 kg) containing 10.8% DHA and 24.0% PUFA was hydrolysed in ethanol / water (90:10 mass ratio) using potassium hydroxide. The pH of the final solution was approximately 14. A saturated urea solution was prepared by mixing 1 kg of urea into 3 L of 90% by mass ethanol / water and then heating to 60° C. This solution was then mixed with the fatty acid hydrolysate solution and allowed to slowly cool. The total solution was then placed in a freezer overnight, and then removed the next day and filtered under gravity to separate the solid urea complex from the filtrate. 6.74 kg of the filtrate was then pumped at 200 bar, at an average mass flow rate of 1.80 kg per hour. The filtrate was mixed with supercritical CO2 at 200 bar and 40° C. before entering the precipitation chamber...

example 2

Recovery of FFA from Urea Filtrates After Two Crystallisations

[0176]This example demonstrates the two-stage concentration of PUFA by sequential urea complexation and supercritical extraction, without intermediate evaporation of ethanol from the FFA.

[0177]The FFA obtained from the first separation stage in Example 1 were added to the ethanol / FFA solution obtained as the second separation stage product (minus a small amount used to determine the FFA content and profile). This solution was then mixed with a saturated urea solution as described in Example 1, with a urea to FFA mass ratio of approximately 1:1. The solution, after cooling and then chilling in the freezer overnight, was filtered. 6.35 kg of the filtrate was then pumped at 200 bar, at an average mass flow rate of 1.69 kg per hour. The filtrate was mixed with supercritical CO2 at 200 bar and 40° C. before entering the precipitation chamber. The supercritical carbon dioxide was pumped at the rate of approximately 12.8 kg per ...

example 3

Recovery of Urea and FFA from Solids

[0181]This example demonstrates the recovery of FFA from urea complexes, and the generation of a dissolved urea fraction that could be recycled for further use. It also demonstrates the separation of AGE from FFA by sequential pressure reduction.

[0182]Urea / FFA complex (1210 g) containing spiny dogfish FFA and AGE at a concentration of 23% by mass was dissolved in a mixture containing 2400 g of ethanol and 1600 g of water. The mixture was heated to 40° C. and stirred gently until all of the solid had dissolved. The homogenous liquid phase was then pumped at 200 bar, at a mass flow rate of approximately 1.52 kg per hour, and mixed with supercritical carbon dioxide at 200 bar and 40° C. before entering the precipitation chamber. The supercritical carbon dioxide was pumped at the rate of approximately 12 kg per hour. A precipitate of mainly water and urea was obtained from the bottom of the precipitation chamber at a rate of approximately 0.88 kg per ...

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Abstract

A process for extracting a wide range of lipophilic compounds from urea-containing solutions is described. The process utilises a near-critical fluid as the extraction solvent. The process is particularly applicable to the extraction of polyunsaturated fatty acids from the filtrate obtained upon urea fractionation, as employed in the processing of fish and other oils. In contrast to known processes, the lipophilic compounds may be extracted without the use of non-food grade solvents, and are suitable for pharmaceutical and cosmetic use.

Description

[0001]This is a nationalization of PCT / NZ03 / 00062 filed Apr. 11, 2003 and published in English.TECHNICAL FIELD[0002]This invention relates to separation technology. A process, which employs a near-critical fluid, for extracting lipophilic compounds from urea-containing solutions is provided.[0003]The process is particularly useful for extracting polyunsaturated fatty acids, or their derivatives, from the filtrate obtained following the urea fractionation of a mixture of fatty acids or their derivatives.BACKGROUND ART[0004]There is a substantial body of research which demonstrates the beneficial effects of polyunsaturated fatty acid (PUFA) consumption in the prevention and / or treatment of a variety of diseases including cardiovascular conditions, inflammatory diseases and some tumours [1, 2]. Therefore there is a demand for PUFA and their derivatives for use as, or in, dietary supplements and pharmaceuticals.[0005]Separation of unsaturated fats and fat derivatives from saturated fats...

Claims

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Application Information

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Patent Type & AuthorityPatents(United States)
IPC IPC(8): C07C51/47C07B63/00C07C51/48C07C57/12C07C67/58C07C403/24C11B1/10C11B7/00C11C1/02C11C1/08C11C3/10
CPCC07C51/48C07C67/58C11B7/005C11C1/025C11C1/08C11C3/10C07C57/12C07C57/03C07C69/587C07C67/56C11B7/00
InventorCATCHPOLE, OWEN JOHNMACKENZIE, ANDREW DOUGLASGREY, JOHN BERTRAM
OwnerIND RES LTD